Page 81 - Application Handbook - Liquid Chromatography
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Application  No.L463
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            n Repeatability                                      mV
            Table 2 and 3 show the relative standard deviations (n=6)   1000
            of retention time and peak area obtained in repeat analysis                   1  n Peaks
            of a mixed histamine and tyramine standard solution (each                        1. Histamine
            1 mg/L). Limits for histamine differ depending on the   750                      2. Tyramine
            country, but in Codex, for example, the limit associated
            with decomposition in fish and fishery products is    500
            100 mg/kg. Good repeatability has been obtained at a
            concentration of about 1/100 of the criterion.                                    2
                                                                  250
             Table 2  Repeatability of Peak   Table 3  Repeatability of Peak
                   Area and Retention     Area and Retention
                   Time of Histamine      Time of Tyramine          0
                                                                     0          5         10        15  min
                   R.t (min)  Peak Area    R.t (min)  Peak Area
              1st   9.962   433,724   1st  11.844  153,458                Fig. 5  Chromatogram of Red Wine
              2nd   9.983   431,874  2nd   11.871  155,582
              3rd   9.967   441,528  3rd   11.858  155,848       mV
              4th   9.962   429,887  4th   11.855  154,509       1000
              5th   9.972   439,560  5th   11.882  151,206                                  ■Peaks
              6th   9.993   434,818  6th   11.911  153,960                                1  1. Histamine
              Ave   9.973   435,232  Ave   11.87  154,094         750                        2. Tyramine
             %RSD   0.12     1.03    %RSD   0.20    1.09
                                                                  500
            n Analysis of Food
            Figures 3 to 8 show examples of analysis of commercial                            2
            fish sauce, wine, and soy sauce. Pretreatment consisted   250
            of preparing a 10-fold dilution using pH 2.2 sodium
            citrate buffer solution, and filtering through a 0.2 µm   0
            pore diameter membrane filter. As for the red wine and   0          5         10        15  min
            white wine, both were spiked with histamine and
            tyramine at 50 mg/L each.                                    Fig. 6  Chromatogram of White Wine

               mV                                                 mV
                                                                 2000
                                       n Peaks
               500                       1. Histamine                                      n Peaks
                                         2. Tyramine                                        1. Histamine
                                                                 1500                       2. Tyramine
                                                                                          1
                                                                                              2
                                                                 1000
               250
                                       1
                                                                  500
                                           2
                0
                  0         5         10         15  min            0  0        5         10        15  min

                      Fig. 3  Chromatogram of Fish Sauce A               Fig. 7  Chromatogram of Soy Sauce A

               mV                                                 mV
                                                                 500
                              n Peaks                                                      n Peaks
               500              1. Histamine                                                1. Histamine
                                2. Tyramine                                                 2. Tyramine

                                                                 250
               250                     1
                                                                                             2
                                           2                                             1
                0                                                  0
                  0         5         10         15  min             0         5         10         15  min

                      Fig. 4  Chromatogram of Fish Sauce B               Fig. 8  Chromatogram of Soy Sauce B
                                                                                                      First Edition: Sep. 2014


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